摘要
以丁酮和1,3-丙二硫醇为原料,采用TiSiW12O40/TiO2作催化剂,合成了一种新型香料化合物2-甲基-2-乙基-1,3-二硫杂环己烷,并用元素分析、IR、1HNMR对其结构进行了表征。采用正交试验研究了影响目标化合物产率的主要因素,得到了优化反应条件:n(丁酮)∶n(1,3-丙二硫醇)=1.1∶1.0,m(催化剂)∶m(1,3-丙二硫醇)=0.04∶1,不需要带水剂,反应3 h,目标产物的收率为87.6%。催化剂无需处理可直接重复使用8次以上。
A new perfume 2 - methyl - 2 - ethyl - 1, 3 - dithiocyclohexane was synthesized using butanone and 1, 3 - dimercaptopropanol as raw materials with TiSiW12O40/TiO2 as catalyst. The structure of the product was characterized by IR,^1HNMR spectra and elemental analysis. Main factors that effecting on the yield of targeted compound were studied through orthogonal designed experiment. The optimal reaction conditions were obtained as follows： the mole ratio of butanone to 1, 3 - dimercaptopropanol 1.1 ： 1.0, mass ratio of catalyst to 1, 3 - dimercaptopropanol 0.04 ： 1, water stripping agent not necessary, reaction time 3 h. The yield of targeted compound achieves 87.6%. The catalyst can be used repeatedly for 8 times without regeneration treatment.
出处
《日用化学工业》
CAS
CSCD
北大核心
2007年第3期212-214,共3页
China Surfactant Detergent & Cosmetics
